摘要
采用改进的QuEChERS方法进行提取和净化,建立了气相色谱-三重四极杆质谱(GC-MS/MS)快速测定酸肉样品中10种挥发性N-亚硝胺类化合物的检测方法。样品经乙腈提取和正己烷除脂后,采用十八烷基硅烷键合硅胶(C18)和N-丙基乙二胺(PSA)混合吸附剂净化,采用DB-WAX色谱柱(30 m×0.25 mm×0.25μm)分离,在选择反应监测(SRM)模式下进行测定,外标法定量。10种N-亚硝胺类化合物在1~100μg/L范围内线性关系良好,相关系数(r)均>0.99。10种N-亚硝胺类化合物的加标回收率为79.8%~115.3%,相对标准偏差(RSD)为0.6%~22.9%(n=6);方法的检出限(LOD,S/N=3)和定量限(LOQ,S/N=10)分别为0.04~0.3μg/kg和0.1~1μg/kg。该法简便快速,灵敏有效,适用于酸肉中N-亚硝胺类化合物的快速筛查和测定。
A rapid gas chromatography-triple quadrupole mass spectrometry(GC-MS/MS)method with modified QuEChERS method was developed for the determination of10volatile N-nitrosamines in sour meats.The samples were extracted with acetonitrile and eliminated the fat with n-hexane.The extracts in acetonitrile layer were purified by octadecyl silane(C18)and primary secondary amine(PSA)sorbents.The N-nitrosamines were determined on a DB-WAX column(30mx0.25mmx0.25pm)by GC-MS/MS in selected reaction monitoring(SRM)mode.The external standard method was used to quantify the N-nitrosamines.The correlation coefficients(r)of the standard calibration curves were greater than0.99in the range of1-100ug/L.The average recoveries ranged from79.8%to115.3%with the relative standard devia-tions(RSDs)from0.6%to22.9%(n=6).The limits of detection(LODs,S/N=3)and limits of quantification(LOQs,S/N=10)were0.04-0.3ug/kg and0.1-1ug/kg,respectively.The developed method is simple,rapid,sensitive and efficient for the screening of the N-nitrosamines in sour meats.
作者
赵庄
许杨彪
刘向红
施晓光
鲁毅翔
ZHAO Zhuang;XU Yangbiao;LIU Xianghong;SHI Xiaoguang;LU Yixian(Guangxi Institute for Food and Drug Control,Nanning 530021,China)
出处
《色谱》
CAS
CSCD
北大核心
2017年第10期1086-1093,共8页
Chinese Journal of Chromatography
基金
广西科技基础条件平台建设项目计划(12-112-01D)~~
